CN108385280B - Composite nanofiber felt and preparation method thereof - Google Patents
Composite nanofiber felt and preparation method thereof Download PDFInfo
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- CN108385280B CN108385280B CN201810087852.7A CN201810087852A CN108385280B CN 108385280 B CN108385280 B CN 108385280B CN 201810087852 A CN201810087852 A CN 201810087852A CN 108385280 B CN108385280 B CN 108385280B
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
Abstract
The invention provides a composite nano fiber felt and a preparation method thereof, which comprises the steps of adding polyhydroxyalkanoate and polyurethane into a mixed solvent of N, N-dimethylacetamide and tetrahydrofuran, then adding polytetrafluoroethylene concentrated solution, and magnetically stirring until the components are completely dissolved; then adding other components into a mixing stirrer, stirring and mixing uniformly, adding the obtained mixed material into a stainless steel reaction kettle, introducing nitrogen and continuously heating to prepare a mixed solution; then mixing and stirring the two solutions to obtain a spinning solution; and (3) feeding the obtained spinning solution into an electrostatic spinning device to prepare an electrospun membrane, drying in a drying oven at 60 ℃ in vacuum to obtain a nano fiber felt, and then carrying out thermal crosslinking treatment on the fiber felt to obtain the composite nano fiber felt. The composite nanofiber felt disclosed by the invention has high mechanical strength and good flexibility, hydrophilicity and chemical resistance.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a composite nanofiber felt and a preparation method thereof.
Background
Electrostatic spinning is widely applied as a special fiber preparation technology, and a nanofiber material with large specific surface area, high porosity and good flexibility can be prepared by adjusting the technological parameters of electrostatic spinning, so that the nanofiber material can be widely applied to various fields of drug delivery, tissue engineering, filter materials, protective clothing, sensors, catalysts and the like. Especially, the nano-fiber drug release system can overcome the defects of the traditional preparation, thereby achieving the requirements of improving the bioavailability, reducing the dosage of the drug and increasing the curative effect of the drug.
The polytetrafluoroethylene has extremely good chemical stability, strong acid resistance, strong alkali resistance, corrosion resistance of various chemical products and wide temperature resistance, so that the polytetrafluoroethylene is an ideal separation filter material in a special separation environment. Polytetrafluoroethylene has excellent hydrophobicity, making it the material of choice for membrane distillation and waterproof breathable materials. However, polytetrafluoroethylene is insoluble in any solvent, so that polytetrafluoroethylene fiber membranes can be processed only by powder metallurgy-like methods. I.e. consisting of a pre-form and a sintered part. At present, some related people have carried out some researches on the preparation, structural performance, application and the like of micron-sized polytetrafluoroethylene fibers, but the researches on nano-sized polytetrafluoroethylene fiber membranes are almost not carried out.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a composite nanofiber felt which is easy to process and good in chemical resistance aiming at the current situation of the prior art. The preparation method is simple and easy to implement and easy to process, and the composite nanofiber felt has high mechanical strength and good flexibility, hydrophilicity and chemical resistance.
A preparation method of a composite nanofiber felt comprises the following steps:
(1) adding polyhydroxyalkanoate and polyurethane into a mixed solvent of N, N-dimethylacetamide and tetrahydrofuran under stirring, continuing stirring for 3-5 h until the mixture is completely swelled, then adding a polytetrafluoroethylene concentrated solution, magnetically stirring until the polytetrafluoroethylene concentrated solution is completely dissolved, and standing for 24h for later use; wherein the mass ratio of the polytetrafluoroethylene to the polyhydroxyalkanoate to the polyurethane is 5-8:10-20: 4-7;
(2) adding glucose, trimethyl phosphite, alkenyl triethoxy silane, ethyl acetate, attapulgite and dilauryl thiodipropionate into a mixing stirrer, and uniformly stirring and mixing to obtain a mixed material; adding the mixed material into a stainless steel reaction kettle, introducing nitrogen, continuously heating, and stirring for reaction for 30-45min to obtain a mixed solution;
(3) mixing and stirring the solution in the step (1) and the mixed solution in the step (2), and then degassing by adopting ultrasonic treatment to obtain a spinning solution; sending the spinning solution into an electrostatic spinning device for electrostatic spinning, drying the collected electrospun fiber membrane in a drying box at the temperature of 60 ℃ in vacuum to obtain a nanofiber felt, and then carrying out thermal crosslinking treatment on the nanofiber felt to obtain a final product; wherein the electrostatic spinning process parameters are as follows: the specification of the injector is 5mL, the inner diameter of a needle is 0.5-0.8 mm, the receiving device is a rotary drum with the surface attached with tinfoil, the rotating speed of the rotary drum is 300-500 rpm, the distance between the needle and the receiving device is 15-25 cm, the spinning voltage is 12-20 kV, the ejection flow rate is 0.8-1.2 mL/h, the humidity is 45-60%, and the spinning temperature is 25-35 ℃; the thermal crosslinking temperature is 110-135 ℃, and the crosslinking time is 30-45 min.
As a further improvement of the invention, the volume ratio of the N, N-dimethylacetamide to the tetrahydrofuran in the step (1) is 4: 1-8: 1.
As a further improvement of the above invention, the present invention is characterized in that: 1-9 parts of glucose, 3-9 parts of trimethyl phosphite, 4-10 parts of alkenyl triethoxy silane, 2-7 parts of ethyl acetate, 5-10 parts of attapulgite and 1-6 parts of dilauryl thiodipropionate in the step (2).
As a further improvement of the invention, the drying time in the step (3) is 24-36 h.
The invention has the beneficial effects that: the composite nanofiber felt comprises polytetrafluoroethylene, polyhydroxyalkanoate, polyurethane, N-dimethylacetamide, tetrahydrofuran, glucose, trimethyl phosphite, alkenyl triethoxy silane, ethyl acetate, attapulgite and dilauryl thiodipropionate, wherein the polytetrafluoroethylene has extremely good chemical stability, strong acid resistance, strong alkali resistance, corrosion resistance of various chemical products and wide temperature resistance, and the polyurethane has excellent elasticity and can endow the products with good rubber elasticity, so that the composite nanofiber felt has great adaptability to external force. In addition, the performances of glucose, trimethyl phosphite, alkenyl triethoxy silane, ethyl acetate, attapulgite and dilauryl thiodipropionate are combined, so that the prepared composite nanofiber felt has high mechanical strength, good flexibility, hydrophilicity and chemical resistance and good application prospect.
Detailed Description
In order to make the objects and advantages of the present invention more apparent, the following description will clearly and completely describe the technical solutions of the present invention with reference to specific embodiments, but the described embodiments of the present invention are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a composite nanofiber felt comprises the following steps:
(1) adding polyhydroxyalkanoate and polyurethane into a mixed solvent of N, N-dimethylacetamide and tetrahydrofuran under stirring, continuing stirring for 3-5 h until the mixture is completely swelled, then adding a polytetrafluoroethylene concentrated solution, magnetically stirring until the polytetrafluoroethylene concentrated solution is completely dissolved, and standing for 24h for later use; wherein the mass ratio of the polytetrafluoroethylene to the polyhydroxyalkanoate to the polyurethane is 5:10:4, and the volume ratio of the N, N-dimethylacetamide to the tetrahydrofuran is 4: 1;
(2) adding glucose, trimethyl phosphite, alkenyl triethoxy silane, ethyl acetate, attapulgite and dilauryl thiodipropionate into a mixing stirrer, and uniformly stirring and mixing to obtain a mixed material; adding the mixed material into a stainless steel reaction kettle, introducing nitrogen, continuously heating, and stirring for reaction for 30min to obtain a mixed solution; wherein, 3 parts of glucose, 5 parts of trimethyl phosphite, 4 parts of alkenyl triethoxy silane, 2 parts of ethyl acetate, 6 parts of attapulgite and 3 parts of dilauryl thiodipropionate;
(3) mixing and stirring the solution in the step (1) and the mixed solution in the step (2), and then degassing by adopting ultrasonic treatment to obtain a spinning solution; sending the spinning solution into an electrostatic spinning device for electrostatic spinning, drying the collected electrospun fiber membrane in a drying box at the temperature of 60 ℃ in vacuum to obtain a nanofiber felt, and then carrying out thermal crosslinking treatment on the nanofiber felt to obtain a final product; wherein the electrostatic spinning process parameters are as follows: the specification of the injector is 5mL, the inner diameter of the needle is 0.5mm, a rotary drum of tinfoil is attached to the surface of the receiving device, the rotating speed of the rotary drum is 300rpm, the distance between the needle and the receiving device is 15cm, the voltage is 12kV, the selected ejection flow rate during electrospinning is 0.8mL/h, the humidity is 45%, and the spinning temperature is 25 ℃; the drying time is 24 hours, the thermal crosslinking temperature is 110 ℃, and the crosslinking time is 30 min.
Example 2
A preparation method of a composite nanofiber felt is characterized by comprising the following steps: the method comprises the following steps:
(1) adding polyhydroxyalkanoate and polyurethane into a mixed solvent of N, N-dimethylacetamide and tetrahydrofuran under stirring, continuing stirring for 3-5 h until the mixture is completely swelled, then adding a polytetrafluoroethylene concentrated solution, magnetically stirring until the polytetrafluoroethylene concentrated solution is completely dissolved, and standing for 24h for later use; wherein the mass ratio of the polytetrafluoroethylene to the polyhydroxyalkanoate to the polyurethane is 8:20:7, and the volume ratio of the N, N-dimethylacetamide to the tetrahydrofuran is 8: 1;
(2) adding glucose, trimethyl phosphite, alkenyl triethoxy silane, ethyl acetate, attapulgite and dilauryl thiodipropionate into a mixing stirrer, and uniformly stirring and mixing to obtain a mixed material; adding the mixed material into a stainless steel reaction kettle, introducing nitrogen, continuously heating, and stirring for reacting for 45min to obtain a mixed solution; wherein 9 parts of glucose, 9 parts of trimethyl phosphite, 10 parts of alkenyl triethoxy silane, 7 parts of ethyl acetate, 10 parts of attapulgite and 6 parts of dilauryl thiodipropionate;
(3) mixing and stirring the solution in the step (1) and the mixed solution in the step (2), and then degassing by adopting ultrasonic treatment to obtain a spinning solution; sending the spinning solution into an electrostatic spinning device for electrostatic spinning, drying the collected electrospun fiber membrane in a drying box at the temperature of 60 ℃ in vacuum to obtain a nanofiber felt, and then carrying out thermal crosslinking treatment on the nanofiber felt to obtain a final product; wherein the electrostatic spinning process parameters are as follows: the specification of the injector is 5mL, the inner diameter of the needle is 0.8mm, a rotary drum of tinfoil is attached to the surface of the receiving device, the rotating speed of the rotary drum is 500rpm, the distance between the needle and the receiving device is 25cm, the voltage is 20kV, the selected ejection flow rate during electrospinning is 1.2mL/h, the humidity is 60%, and the spinning temperature is 35 ℃; the drying time is 36h, the thermal crosslinking temperature is 135 ℃, and the crosslinking time is 45 min.
Claims (4)
1. A preparation method of a composite nanofiber felt is characterized by comprising the following steps: the method comprises the following steps:
(1) adding polyhydroxyalkanoate and polyurethane into a mixed solvent of N, N-dimethylacetamide and tetrahydrofuran under stirring, continuing stirring for 3-5 h until the mixture is completely swelled, then adding a polytetrafluoroethylene concentrated solution, magnetically stirring until the polytetrafluoroethylene concentrated solution is completely dissolved, and standing for 24h for later use; wherein the mass ratio of the polytetrafluoroethylene to the polyhydroxyalkanoate to the polyurethane is 5-8:10-20: 4-7;
(2) adding glucose, trimethyl phosphite, alkenyl triethoxy silane, ethyl acetate, attapulgite and dilauryl thiodipropionate into a mixing stirrer, and uniformly stirring and mixing to obtain a mixed material; adding the mixed material into a stainless steel reaction kettle, introducing nitrogen, continuously heating, and stirring for reaction for 30-45min to obtain a mixed solution;
(3) mixing and stirring the solution in the step (1) and the mixed solution in the step (2), and then degassing by adopting ultrasonic treatment to obtain a spinning solution; sending the spinning solution into an electrostatic spinning device for electrostatic spinning, drying the collected electrospun fiber membrane in a drying box at the temperature of 60 ℃ in vacuum to obtain a nanofiber felt, and then carrying out thermal crosslinking treatment on the nanofiber felt to obtain a final product; wherein the electrostatic spinning process parameters are as follows: the specification of the injector is 5mL, the inner diameter of a needle is 0.5-0.8 mm, the receiving device is a rotary drum with the surface attached with tinfoil, the rotating speed of the rotary drum is 300-500 rpm, the distance between the needle and the receiving device is 15-25 cm, the spinning voltage is 12-20 kV, the ejection flow rate is 0.8-1.2 mL/h, the humidity is 45-60%, and the spinning temperature is 25-35 ℃; the thermal crosslinking temperature is 110-135 ℃, and the crosslinking time is 30-45 min.
2. The method of preparing a composite nanofiber mat as claimed in claim 1, wherein: the volume ratio of the N, N-dimethylacetamide to the tetrahydrofuran in the step (1) is 4: 1-8: 1.
3. The method of preparing a composite nanofiber mat as claimed in claim 1, wherein: 1-9 parts of glucose, 3-9 parts of trimethyl phosphite, 4-10 parts of alkenyl triethoxy silane, 2-7 parts of ethyl acetate, 5-10 parts of attapulgite and 1-6 parts of dilauryl thiodipropionate in the step (2).
4. The method of preparing a composite nanofiber mat as claimed in claim 1, wherein: the drying time in the step (3) is 24-36 h.
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| CN201810087852.7A CN108385280B (en) | 2018-01-30 | 2018-01-30 | Composite nanofiber felt and preparation method thereof |
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| CN108385280B true CN108385280B (en) | 2020-06-16 |
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| CA2935128A1 (en) * | 2013-12-27 | 2015-07-02 | Neograft Technologies, Inc. | Artificial graft devices and related systems and methods |
| CN106012102A (en) * | 2014-11-07 | 2016-10-12 | 蔡留凤 | Biomedical electrospun film |
| KR101794003B1 (en) * | 2015-11-26 | 2017-11-08 | 한국세라믹기술원 | Method of manufacturing porous nanofiber composite using electricity spinning |
| CN105839295B (en) * | 2016-06-17 | 2019-04-30 | 合肥市易远新材料有限公司 | A kind of preparation method of antibiotic fiber film |
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Effective date of registration: 20200519 Address after: 512000 Lianfeng science and Technology Industrial Park, Shixing County, Shaoguan City, Guangdong Province Applicant after: Lianfeng fiber products (Shixing) Co., Ltd Address before: 314299 Xinhua Apartment, Danghu Street, Pinghu City, Jiaxing City, Zhejiang Province Applicant before: PINGHU YIFANJIA BAG Co.,Ltd. |
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